CN109133830A - A kind of preparation method of ardealite based self-leveling material - Google Patents

A kind of preparation method of ardealite based self-leveling material Download PDF

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CN109133830A
CN109133830A CN201811130444.1A CN201811130444A CN109133830A CN 109133830 A CN109133830 A CN 109133830A CN 201811130444 A CN201811130444 A CN 201811130444A CN 109133830 A CN109133830 A CN 109133830A
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parts
ardealite
calcium
water
based self
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CN109133830B (en
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战英权
马俊杰
朱东东
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Guizhou Tianchen Sanjiang building materials Co., Ltd
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Foshan Qi An Construction Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/14Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
    • C04B28/145Calcium sulfate hemi-hydrate with a specific crystal form
    • C04B28/146Calcium sulfate hemi-hydrate with a specific crystal form alpha-hemihydrate
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The invention discloses a kind of preparation methods of ardealite based self-leveling material, belong to building material technical field.The present invention first pulverizes and sieves ardealite, it obtains and tentatively refines ardealite, after ardealite and water mixing will tentatively be refined again, calcium plaster is made in chilled thaw cycles, and is diluted with water to calcium plaster, then by it after graphene oxide, dehydrated alcohol and oleic acid are uniformly mixed, freezing squeezing, it thaws, it is dry, squeezing material must be dried;Material and absolute ethyl alcohol and stirring are squeezed after mixing for dry again, then the concentrated sulfuric acid is added dropwise, after constant temperature is stirred to react, adds calcium salt soln, and adjusts pH to alkalinity, after hydro-thermal is stirred to react, are filtered, washing and drying obtain modified ardealite;It is stirred with anhydrite, semi-hydrated gypsum, cement, quartz sand, calcium sulphate retarder and water-reducing agent again, is discharged, is packed to get ardealite based self-leveling material.Gained ardealite based self-leveling material of the invention has excellent mobile performance and intensity.

Description

A kind of preparation method of ardealite based self-leveling material
Technical field
The invention discloses a kind of preparation methods of ardealite based self-leveling material, belong to building material technical field.
Background technique
Gravity flowing levelling mortar has excellent workability, can save labour, construction efficiency is improved, in building decoration and fitment It has a wide range of applications in engineering.Ground is one kind using inorganic coagulation material or organic material as substrate with gravity flowing levelling mortar, with Building ground self-leveling material made of aggregate and a variety of composition of concrete admixture.Gravity flowing levelling mortar include inorganic system's gravity flowing levelling mortar with Organic system gravity flowing levelling mortar, inorganic system's gravity flowing levelling mortar include cement-based self-leveling mortar and gypsum based self-leveling mortar again.From The maximum of levelling mortar is characterized in thering is good mobility, can flow freely formation under the action of self weight and self-expanding stress Horizontal plane, thus the accurate levelling ground of large area in a short time, this brings very big help to the application of some engineering material.
Gypsum based self-leveling mortar is to be aided with the ground of aggregate, other cementitious materials and additive using gypsum as base-material Self-leveling material has speed of application fast, short construction period, simple process, insulated fire performance good and feel snugness etc. Advantage.Gypsum base-material for gypsum based self-leveling mortar mainly has α high strength gypsum, β gypsum etc., can be by the natural gypsum, desulfurization Gypsum, ardealite calcining are prepared.Currently, the gypsum based self-leveling mortar intensity prepared using α high strength gypsum as base-material compared with Good, over dry flexural strength is up to 10MPa, and over dry compression strength is up to 29MPa.But since gypsum based self-leveling mortar is a kind of gas Hydraulic cement, intensity and cement-based self-leveling mortar still have larger gap, therefore, improve the strong of gypsum based self-leveling mortar Degree becomes urgent problem.When gravity flowing levelling mortar is as floor material, surface is the direct abrasion for bearing traffic above-ground Works.The thinner thickness of gravity flowing levelling mortar, in the case where ground layer is solid, carried active force is concentrated mainly on table Face.The problem of ardealite based self-leveling material traditional at present can not be further increased there is also mobile performance and intensity, therefore It also needs to study it.
Summary of the invention
The present invention solves the technical problem of: for traditional ardealite based self-leveling material mobile performance and intensity without The problem of method further increases provides a kind of preparation method of ardealite based self-leveling material.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
(1) after crushing ardealite, 60 meshes are crossed, obtain tentatively refinement ardealite;
(2) it is in mass ratio after 1:3~1:5 is uniformly mixed by preliminary refinement ardealite and water, chilled thaw cycles 8~ 10 times, calcium plaster is obtained, then by gained calcium plaster and water is in mass ratio 1:5~1:10 mixed diluting, obtains dilution calcium plaster;
(3) according to parts by weight, 20~30 parts of dilution calcium plasters are successively taken, 10~15 parts of graphene oxides, 20~30 parts anhydrous Ethyl alcohol, 20~30 parts of oleic acid, after being uniformly mixed, freezing squeezing is thawed, dry, must dry squeezing material;
(4) according to parts by weight, 60~80 parts of freezing squeezings is successively taken to expect, 3~5 parts of concentrated sulfuric acids, 40~50 parts of calcium salt solns, 30 First after mixing by dry squeezing material and absolute ethyl alcohol and stirring, then the concentrated sulfuric acid is added dropwise in~40 parts of dehydrated alcohols, and constant temperature stirring is anti- Ying Hou adds calcium salt soln, and adjusts pH to alkalinity, and after hydro-thermal is stirred to react, filtering washs and dry, obtains modified phosphorus stone Cream;
(5) according to parts by weight, 80~100 parts of anhydrite, 200~300 parts of modified ardealites, 200~300 parts of α-half are successively taken Water gypsum, 30~50 parts of cement, 80~100 parts of quartz sands, 3~5 parts of calcium sulphate retarders, 2~4 parts of water-reducing agents are stirred Even, discharging is packed to get ardealite based self-leveling material.
Step (2) described freeze-thaw are as follows: after freezing 6~8h under the conditions of being -20~-18 DEG C in temperature, in microwave power For the 45~60min that thaws under the conditions of 300~400W.
Step (4) described concentrated sulfuric acid is the concentrated sulfuric acid that mass fraction is 95~98%.
Step (4) described calcium salt soln is the calcium salt soln that mass fraction is 8~10%;The calcium salt is calcium nitrate, chlorination Any one in calcium.
Step (4) the adjusting pH adjusts pH to 9.0~9.5 to alkalinity.
Step (5) cement is ordinary portland cement, portland slag cement, fine coal grey matter portland cement, fire Any one in the grey matter portland cement of mountain.
Step (5) calcium sulphate retarder is borax, citric acid, malic acid, any one in sodium polyphosphate.
Step (5) water-reducing agent is sodium lignin sulfonate, TH-928 poly carboxylic acid series water reducer, YZ-1 naphthalene series high-efficiency diminishing Any one in agent.
The beneficial effects of the present invention are:
(1) technical solution of the present invention makes ardealite raw material by preliminary refinement first with mechanical crushing, then will tentatively refine Ardealite and water mixing, enter moisture penetration in ardealite pore structure, in process of osmosis, can make to have not product strength The water-solubility impurity of good influence dissolves out, and forms hole at the position for occupying script water-solubility impurity after dissolution, holds that moisture more Inside easily is penetrated into, then cooperates freeze-thaw circulation, in refrigerating process, the moisture in hole, which freezes, occurs volume expansion, To make ardealite pore structure widen, in course of defrosting, moisture can further deeply and permeate, and repeatedly freezed and thawed Cyclic process makes ardealite hole avalanche because of the change of water state, and ardealite is further refined, and pore structure is more It is abundant;
(2) technical solution of the present invention is by the way that dilute the moisture in calcium plaster as water phase, oleic acid is oily phase, is aided with graphite oxide Alkene contains hydrophobic region and hydrophilic area in graphene oxide molecular structure simultaneously, causes it with good emulsifiability, thus Under graphene oxide auxiliary, microemulsion is formed, and having silver is that graphene oxide has good absorption property, adsorbable refinement Ardealite is at oil-water interface, and in subsequent refrigerating process, the moisture in the oleic acid and water phase of oily phase solidifies, and Under mechanical pressure, hydrogenesis at ice crystal fragmentation, cause ardealite further to refine, can be common with graphene oxide after refinement It is wrapped up by oleic acid, to form core-shell structure, the presence of oleic acid layer, the ardealite generation after can effectively avoid refinement is rolled into a ball again It is poly-;
(3) dry squeezing material and absolute ethyl alcohol and stirring are reacted, were being reacted using the concentrated sulfuric acid as catalyst by technical solution of the present invention Cheng Zhong, on the one hand but esterification occurs for surface coated oleic acid and dehydrated alcohol to the oleate that wakes, the oleic acid of generation Ester has good surface-active, can not only ensure the fine dispersion of refinement ardealite during the preparation process, also help reduction The viscosity of product in use, improves the mobility of product, is conducive to product in the wetting of matrix surface and sprawls;It is another Aspect, contained phosphorus pentoxide can be under sulphuric acid catalysis effect and dehydrated alcohol react to form phosphatide in ardealite, and phosphatide exists After subsequent alkaline environment issues unboiled water solution, and the calcium binding that dissociates in system, so that it be made to be changed into calcium hydroxy phosphate crystal, Once having calcium hydroxy phosphate nucleus to be formed can be fixed by graphene oxide absorption in system, its size is made to be maintained at nanoscale, The fine dispersion of ardealite, graphene oxide and calcium hydroxy phosphate in system, after having ensured that product solidifies in use Firm film layer can be formed in matrix surface, the strength character of product is enable effectively to enhance.
Specific embodiment
Ardealite is poured into pulverizer, 60 meshes are smashed it through, obtains tentatively refinement ardealite;Gained is tentatively refined again Ardealite and water are that 1:3~1:5 mixing is poured into No. 1 batch mixer in mass ratio, are stirred with blender with 600~800r/min revolving speed After mixing 2~4h of mixing, 6~8h is freezed under the conditions of being -20~-18 DEG C in temperature by material in No. 1 batch mixer, then at microwave power Under the conditions of 300~400W, thaw 45~60min, after such freeze-thaw circulation 8~10 times, collects last time defrosting object Material, obtains calcium plaster, then by gained calcium plaster and water is in mass ratio 1:5~1:10 mixed diluting, obtains dilution calcium plaster;By weight Number meter, successively takes 20~30 parts of dilution calcium plasters, 10~15 parts of graphene oxides, 20~30 parts of dehydrated alcohols, and 20~30 parts Oleic acid, mixing is poured into No. 2 batch mixers, after being stirred 45~60min with 1000~1200r/min revolving speed, by No. 2 batch mixers Middle material 2~3min of liquid nitrogen frozen obtains frozen materials, then gained frozen materials is transferred in squeezer, in pressure be 1.7~ 20~30s, pressure release are squeezed in pressure maintaining under the conditions of 2.0MPa, and discharging must squeeze material, then gained squeezing material is turned after natural thaw Enter in baking oven, dries under the conditions of being 75~85 DEG C in temperature to constant weight, discharging, squeezing material must be dried;According to parts by weight, successively It takes 60~80 parts of freezings to squeeze to expect, 3~5 parts of concentrated sulfuric acids, 40~50 parts of calcium salt solns, 30~40 parts of dehydrated alcohols will first be dried Squeezing material and dehydrated alcohol pour into water heating kettle, after being stirred 45~60min with blender with 600~800r/min revolving speed, The concentrated sulfuric acid is added dropwise again, after the concentrated sulfuric acid is added dropwise, in temperature be 80~85 DEG C, it is permanent under the conditions of revolving speed is 400~600r/min After temperature is stirred to react 3~5h, then calcium salt soln is added into water heating kettle, after being added to calcium salt dissolution, adjusts in water heating kettle Material pH to 9.0~9.5, then water heating kettle is closed, it is 165~170 DEG C in temperature, revolving speed is 400~500r/min condition Under, after hydro-thermal is stirred to react 6~8h, water heating kettle is opened, filtering obtains filter cake, and be washed with deionized filter cake 3~5 times, then will Filter cake after washing is transferred in baking oven, is dried under the conditions of being 160~165 DEG C in temperature to constant weight, discharging obtains modified ardealite; According to parts by weight, 80~100 parts of anhydrite are successively taken, 200~300 parts of modified ardealites, 200~300 parts of alpha-semi water plaster stones, 30~50 parts of cement, 20~30 parts of redispersible rubber powders, 80~100 parts of quartz sands, 3~5 parts of calcium sulphate retarders, 2~4 parts subtract Aqua pours into No. 3 batch mixers, under the conditions of revolving speed is 400~500r/min, after being stirred 3~5h, discharges, packaging, i.e., Obtain ardealite based self-leveling material.The concentrated sulfuric acid is the concentrated sulfuric acid that mass fraction is 95~98%.The calcium salt soln is quality The calcium salt soln that score is 8~10%;The calcium salt is calcium nitrate, any one in calcium chloride.The cement is common silicic acid Salt cement, portland slag cement, fine coal grey matter portland cement, any one in Portland pozzolana cement.It is described Calcium sulphate retarder is borax, citric acid, malic acid, any one in sodium polyphosphate.The water-reducing agent is lignin sulfonic acid Sodium, any one in TH-928 poly carboxylic acid series water reducer, YZ-1 naphthalene series high-efficiency water-reducing agent.
Ardealite is poured into pulverizer, 60 meshes are smashed it through, obtains tentatively refinement ardealite;Gained is tentatively refined again Ardealite and water are that 1:5 mixing is poured into No. 1 batch mixer in mass ratio, are stirred 4h with blender with 800r/min revolving speed Afterwards, by material in No. 1 batch mixer in temperature be -18 DEG C under the conditions of freeze 8h, then at microwave power be 400W under the conditions of, thaw 60min after such freeze-thaw circulation 10 times, collects last time defrosting material, obtains calcium plaster, then by gained calcium plaster and water It is in mass ratio 1:10 mixed diluting, obtains dilution calcium plaster;According to parts by weight, 30 parts of dilution calcium plasters, 15 parts of oxygen are successively taken Graphite alkene, 30 parts of dehydrated alcohols, 30 parts of oleic acid, mixing are poured into No. 2 batch mixers, are stirred with 1200r/min revolving speed After 60min, by material liquid nitrogen frozen 3min in No. 2 batch mixers, frozen materials are obtained, then gained frozen materials are transferred to squeezer In, 30s, pressure release are squeezed in pressure maintaining under the conditions of pressure is 2.0MPa, and discharging after natural thaw, must squeeze material, then gained is pressed It squeezes material to be transferred in baking oven, dries under the conditions of being 85 DEG C in temperature to constant weight, discharging, squeezing material must be dried;According to parts by weight, according to It is secondary to take 80 parts of freezing squeezing material, 5 parts of concentrated sulfuric acids, 50 parts of calcium salt solns, 40 parts of dehydrated alcohols, first by dry squeezing material and anhydrous second Alcohol pours into water heating kettle, after being stirred 60min with blender with 800r/min revolving speed, then the concentrated sulfuric acid is added dropwise, and drips to the concentrated sulfuric acid After adding, it is 85 DEG C in temperature, under the conditions of revolving speed is 600r/min, after constant temperature is stirred to react 5h, then is added into water heating kettle Calcium salt soln adjusts material pH to 9.5 in water heating kettle, then water heating kettle is closed, in temperature after being added to calcium salt dissolution Be 170 DEG C, revolving speed be 500r/min under the conditions of, after hydro-thermal is stirred to react 8h, open water heating kettle, filtering, obtain filter cake, and spend from Sub- water washing filter cake 5 times, then the filter cake after washing is transferred in baking oven is dried under the conditions of being 165 DEG C in temperature to constant weight, out Material, obtains modified ardealite;According to parts by weight, 100 parts of anhydrite, 300 parts of modified ardealites, 300 parts of α-half water stones are successively taken Cream, 50 parts of cement, 30 parts of redispersible rubber powders, 100 parts of quartz sands, 5 parts of calcium sulphate retarders, 4 parts of water-reducing agents pour into No. 3 and mix In material machine, under the conditions of revolving speed is 500r/min, after being stirred 5h, discharging is packed to get ardealite based self-leveling material. The concentrated sulfuric acid is the concentrated sulfuric acid that mass fraction is 98%.The calcium salt soln is the calcium salt soln that mass fraction is 10%;It is described Calcium salt is calcium nitrate.The cement is ordinary portland cement.The calcium sulphate retarder is borax.The water-reducing agent is lignin Sodium sulfonate.
Ardealite is poured into pulverizer, 60 meshes are smashed it through, obtains tentatively refinement ardealite;Gained is tentatively refined again Ardealite and water are 1:10 mixed diluting in mass ratio, obtain dilution calcium plaster;According to parts by weight, 30 parts of dilution gypsum are successively taken Slurry, 15 parts of graphene oxides, 30 parts of dehydrated alcohols, 30 parts of oleic acid, mixing are poured into No. 2 batch mixers, are stirred with 1200r/min revolving speed After mixing mixing 60min, by material liquid nitrogen frozen 3min in No. 2 batch mixers, frozen materials are obtained, then gained frozen materials are transferred to In squeezer, 30s, pressure release are squeezed in pressure maintaining under the conditions of pressure is 2.0MPa, and discharging must squeeze material, then will after natural thaw Gained squeezing material is transferred in baking oven, is dried under the conditions of being 85 DEG C in temperature to constant weight, discharging, must be dried squeezing material;By weight Number meter successively takes 80 parts of freezing squeezing material, 5 parts of concentrated sulfuric acids, 50 parts of calcium salt solns, 40 parts of dehydrated alcohols, first by dry squeezing material It is poured into water heating kettle with dehydrated alcohol, after being stirred 60min with blender with 800r/min revolving speed, then the concentrated sulfuric acid is added dropwise, to After the concentrated sulfuric acid is added dropwise, in temperature be 85 DEG C, under the conditions of revolving speed is 600r/min, after constant temperature is stirred to react 5h, then to hydro-thermal Calcium salt soln is added in kettle, after being added to calcium salt dissolution, adjusts material pH to 9.5 in water heating kettle, then water heating kettle is close It closes, is 170 DEG C in temperature, under the conditions of revolving speed is 500r/min, after hydro-thermal is stirred to react 8h, opens water heating kettle, filtering must filter Cake, and be washed with deionized filter cake 5 times, then the filter cake after washing is transferred in baking oven, it is dry under the conditions of being 165 DEG C in temperature To constant weight, discharging obtains modified ardealite;According to parts by weight, 100 parts of anhydrite are successively taken, 300 parts of modified ardealites, 300 parts Alpha-semi water plaster stone, 50 parts of cement, 30 parts of redispersible rubber powders, 100 parts of quartz sands, 5 parts of calcium sulphate retarders, 4 parts of water-reducing agents, Enter in No. 3 batch mixers, under the conditions of revolving speed is 500r/min, after being stirred 5h, discharging, packaging is to get the gravity flow of ardealite base Flat material.The concentrated sulfuric acid is the concentrated sulfuric acid that mass fraction is 98%.The calcium salt soln is that the calcium salt that mass fraction is 10% is molten Liquid;The calcium salt is calcium nitrate.The cement is ordinary portland cement.The calcium sulphate retarder is borax.The water-reducing agent For sodium lignin sulfonate.
Ardealite is poured into pulverizer, 60 meshes are smashed it through, obtains tentatively refinement ardealite;Gained is tentatively refined again Ardealite and water are that 1:5 mixing is poured into No. 1 batch mixer in mass ratio, are stirred 4h with blender with 800r/min revolving speed Afterwards, by material in No. 1 batch mixer in temperature be -18 DEG C under the conditions of freeze 8h, then at microwave power be 400W under the conditions of, thaw 60min after such freeze-thaw circulation 10 times, collects last time defrosting material, obtains calcium plaster, then by gained calcium plaster and water It is in mass ratio 1:10 mixed diluting, obtains dilution calcium plaster;According to parts by weight, 30 parts of dilution calcium plasters, 15 parts of creams are successively taken Agent OP-10,30 parts of dehydrated alcohols, 30 parts of oleic acid, mixing are poured into No. 2 batch mixers, are stirred with 1200r/min revolving speed After 60min, by material liquid nitrogen frozen 3min in No. 2 batch mixers, frozen materials are obtained, then gained frozen materials are transferred to squeezer In, 30s, pressure release are squeezed in pressure maintaining under the conditions of pressure is 2.0MPa, and discharging after natural thaw, must squeeze material, then gained is pressed It squeezes material to be transferred in baking oven, dries under the conditions of being 85 DEG C in temperature to constant weight, discharging, squeezing material must be dried;According to parts by weight, according to It is secondary to take 80 parts of freezing squeezing material, 5 parts of concentrated sulfuric acids, 50 parts of calcium salt solns, 40 parts of dehydrated alcohols, first by dry squeezing material and anhydrous second Alcohol pours into water heating kettle, after being stirred 60min with blender with 800r/min revolving speed, then the concentrated sulfuric acid is added dropwise, and drips to the concentrated sulfuric acid After adding, it is 85 DEG C in temperature, under the conditions of revolving speed is 600r/min, after constant temperature is stirred to react 5h, then is added into water heating kettle Calcium salt soln adjusts material pH to 9.5 in water heating kettle, then water heating kettle is closed, in temperature after being added to calcium salt dissolution Be 170 DEG C, revolving speed be 500r/min under the conditions of, after hydro-thermal is stirred to react 8h, open water heating kettle, filtering, obtain filter cake, and spend from Sub- water washing filter cake 5 times, then the filter cake after washing is transferred in baking oven is dried under the conditions of being 165 DEG C in temperature to constant weight, out Material, obtains modified ardealite;According to parts by weight, 100 parts of anhydrite, 300 parts of modified ardealites, 300 parts of α-half water stones are successively taken Cream, 50 parts of cement, 30 parts of redispersible rubber powders, 100 parts of quartz sands, 5 parts of calcium sulphate retarders, 4 parts of water-reducing agents pour into No. 3 and mix In material machine, under the conditions of revolving speed is 500r/min, after being stirred 5h, discharging is packed to get ardealite based self-leveling material. The concentrated sulfuric acid is the concentrated sulfuric acid that mass fraction is 98%.The calcium salt soln is the calcium salt soln that mass fraction is 10%;It is described Calcium salt is calcium nitrate.The cement is ordinary portland cement.The calcium sulphate retarder is borax.The water-reducing agent is lignin Sodium sulfonate.
Ardealite is poured into pulverizer, 60 meshes are smashed it through, obtains tentatively refinement ardealite;Gained is tentatively refined again Ardealite and water are that 1:5 mixing is poured into No. 1 batch mixer in mass ratio, are stirred 4h with blender with 800r/min revolving speed Afterwards, by material in No. 1 batch mixer in temperature be -18 DEG C under the conditions of freeze 8h, then at microwave power be 400W under the conditions of, thaw 60min after such freeze-thaw circulation 10 times, collects last time defrosting material, obtains calcium plaster, then by gained calcium plaster and water It is in mass ratio 1:10 mixed diluting, obtains dilution calcium plaster;According to parts by weight, 30 parts of dilution calcium plasters, 15 parts of oxygen are successively taken Graphite alkene, 30 parts of dehydrated alcohols, mixing is poured into No. 2 batch mixers, after being stirred 60min with 1200r/min revolving speed, by 2 Material liquid nitrogen frozen 3min in number batch mixer, obtains frozen materials, then gained frozen materials are transferred in squeezer, is in pressure 30s, pressure release are squeezed in pressure maintaining under the conditions of 2.0MPa, and discharging must squeeze material, then gained squeezing material is transferred to baking after natural thaw In case, dries under the conditions of being 85 DEG C in temperature to constant weight, discharging, squeezing material must be dried;According to parts by weight, successively take 80 parts it is cold Freeze squeezing to expect, 5 parts of concentrated sulfuric acids, 50 parts of calcium salt solns, 40 parts of dehydrated alcohols, dry squeezing material and dehydrated alcohol are first poured into hydro-thermal In kettle, after being stirred 60min with blender with 800r/min revolving speed, then the concentrated sulfuric acid is added dropwise, after the concentrated sulfuric acid is added dropwise, in Temperature is 85 DEG C, under the conditions of revolving speed is 600r/min, after constant temperature is stirred to react 5h, then calcium salt soln is added into water heating kettle, to After calcium salt dissolution is added, adjust material pH to 9.5 in water heating kettle, then it is water heating kettle is closed, in temperature be 170 DEG C, revolving speed Under the conditions of 500r/min, after hydro-thermal is stirred to react 8h, water heating kettle is opened, filtering obtains filter cake, and filter cake is washed with deionized 5 times, then the filter cake after washing is transferred in baking oven, it dries under the conditions of being 165 DEG C in temperature to constant weight, discharging obtains modified phosphorus stone Cream;According to parts by weight, 100 parts of anhydrite are successively taken, 300 parts of modified ardealites, 300 parts of alpha-semi water plaster stones, 50 parts of cement, 30 Part redispersible rubber powder, 100 parts of quartz sands, 5 parts of calcium sulphate retarders, 4 parts of water-reducing agents pour into No. 3 batch mixers, are in revolving speed Under the conditions of 500r/min, after being stirred 5h, discharging is packed to get ardealite based self-leveling material.The concentrated sulfuric acid is quality The concentrated sulfuric acid that score is 98%.The calcium salt soln is the calcium salt soln that mass fraction is 10%;The calcium salt is calcium nitrate.It is described Cement is ordinary portland cement.The calcium sulphate retarder is borax.The water-reducing agent is sodium lignin sulfonate.
Ardealite is poured into pulverizer, 60 meshes are smashed it through, obtains tentatively refinement ardealite;Gained is tentatively refined again Ardealite and water are that 1:5 mixing is poured into No. 1 batch mixer in mass ratio, are stirred 4h with blender with 800r/min revolving speed Afterwards, by material in No. 1 batch mixer in temperature be -18 DEG C under the conditions of freeze 8h, then at microwave power be 400W under the conditions of, thaw 60min after such freeze-thaw circulation 10 times, collects last time defrosting material, obtains calcium plaster, then by gained calcium plaster and water It is in mass ratio 1:10 mixed diluting, obtains dilution calcium plaster;According to parts by weight, 30 parts of dilution calcium plasters, 15 parts of oxygen are successively taken Graphite alkene, 30 parts of dehydrated alcohols, 30 parts of oleic acid, mixing are poured into No. 2 batch mixers, are stirred with 1200r/min revolving speed After 60min, by material liquid nitrogen frozen 3min in No. 2 batch mixers, frozen materials are obtained, then gained frozen materials are transferred to squeezer In, 30s, pressure release are squeezed in pressure maintaining under the conditions of pressure is 2.0MPa, and discharging after natural thaw, must squeeze material, then gained is pressed It squeezes material to be transferred in baking oven, dries under the conditions of being 85 DEG C in temperature to constant weight, discharging, squeezing material must be dried;According to parts by weight, according to Secondary that 80 parts of freezing squeezings is taken to expect, dry squeezing material and dehydrated alcohol are first poured into water heating kettle by 5 parts of concentrated sulfuric acids, 40 parts of dehydrated alcohols In, after being stirred 60min with blender with 800r/min revolving speed, then the concentrated sulfuric acid is added dropwise, after the concentrated sulfuric acid is added dropwise, Yu Wen Degree is 85 DEG C, under the conditions of revolving speed is 600r/min, after constant temperature is stirred to react 5h, opens water heating kettle, filtering obtains filter cake, and spend Ion water washing filter cake 5 times, then the filter cake after washing is transferred in baking oven is dried under the conditions of being 165 DEG C in temperature to constant weight, out Material, obtains modified ardealite;According to parts by weight, 100 parts of anhydrite, 300 parts of modified ardealites, 300 parts of α-half water stones are successively taken Cream, 50 parts of cement, 30 parts of redispersible rubber powders, 100 parts of quartz sands, 5 parts of calcium sulphate retarders, 4 parts of water-reducing agents pour into No. 3 and mix In material machine, under the conditions of revolving speed is 500r/min, after being stirred 5h, discharging is packed to get ardealite based self-leveling material. The concentrated sulfuric acid is the concentrated sulfuric acid that mass fraction is 98%.The cement is ordinary portland cement.The calcium sulphate retarder is boron Sand.The water-reducing agent is sodium lignin sulfonate.
Comparative example: the self-leveling material of Jiangsu environmental science and technology Co., Ltd production.
1 to 5 gained self-leveling material of example and comparative example product are subjected to performance detection, the specific detection method is as follows:
Performance detection is carried out to above-mentioned self-leveling material according to JC/T985 standard, specific testing result is as shown in table 1:
Table 1: performance detection table
By 1 testing result of table it is found that present invention gained ardealite based self-leveling material has excellent mobile performance and intensity.

Claims (8)

1. a kind of preparation method of ardealite based self-leveling material, it is characterised in that specific preparation step are as follows:
(1) after crushing ardealite, 60 meshes are crossed, obtain tentatively refinement ardealite;
(2) it is in mass ratio after 1:3~1:5 is uniformly mixed by preliminary refinement ardealite and water, chilled thaw cycles 8~ 10 times, calcium plaster is obtained, then by gained calcium plaster and water is in mass ratio 1:5~1:10 mixed diluting, obtains dilution calcium plaster;
(3) according to parts by weight, 20~30 parts of dilution calcium plasters are successively taken, 10~15 parts of graphene oxides, 20~30 parts anhydrous Ethyl alcohol, 20~30 parts of oleic acid, after being uniformly mixed, freezing squeezing is thawed, dry, must dry squeezing material;
(4) according to parts by weight, 60~80 parts of freezing squeezings is successively taken to expect, 3~5 parts of concentrated sulfuric acids, 40~50 parts of calcium salt solns, 30 First after mixing by dry squeezing material and absolute ethyl alcohol and stirring, then the concentrated sulfuric acid is added dropwise in~40 parts of dehydrated alcohols, and constant temperature stirring is anti- Ying Hou adds calcium salt soln, and adjusts pH to alkalinity, and after hydro-thermal is stirred to react, filtering washs and dry, obtains modified phosphorus stone Cream;
(5) according to parts by weight, 80~100 parts of anhydrite, 200~300 parts of modified ardealites, 200~300 parts of α-half are successively taken Water gypsum, 30~50 parts of cement, 80~100 parts of quartz sands, 3~5 parts of calcium sulphate retarders, 2~4 parts of water-reducing agents are stirred Even, discharging is packed to get ardealite based self-leveling material.
2. a kind of preparation method of ardealite based self-leveling material according to claim 1, it is characterised in that step (2) institute State freeze-thaw are as follows: after freezing 6~8h under the conditions of being -20~-18 DEG C in temperature, under the conditions of microwave power is 300~400W Thaw 45~60min.
3. a kind of preparation method of ardealite based self-leveling material according to claim 1, it is characterised in that step (4) institute Stating the concentrated sulfuric acid is the concentrated sulfuric acid that mass fraction is 95~98%.
4. a kind of preparation method of ardealite based self-leveling material according to claim 1, it is characterised in that step (4) institute Stating calcium salt soln is the calcium salt soln that mass fraction is 8~10%;The calcium salt is calcium nitrate, any one in calcium chloride.
5. a kind of preparation method of ardealite based self-leveling material according to claim 1, it is characterised in that step (4) institute Stating and adjusting pH to alkalinity is to adjust pH to 9.0~9.5.
6. a kind of preparation method of ardealite based self-leveling material according to claim 1, it is characterised in that step (5) institute Cement is stated as in ordinary portland cement, portland slag cement, fine coal grey matter portland cement, Portland pozzolana cement Any one.
7. a kind of preparation method of ardealite based self-leveling material according to claim 1, it is characterised in that step (5) institute Calcium sulphate retarder is stated as any one in borax, citric acid, malic acid, sodium polyphosphate.
8. a kind of preparation method of ardealite based self-leveling material according to claim 1, it is characterised in that step (5) institute Stating water-reducing agent is sodium lignin sulfonate, any one in TH-928 poly carboxylic acid series water reducer, YZ-1 naphthalene series high-efficiency water-reducing agent.
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CN110818297A (en) * 2019-10-28 2020-02-21 昆明理工大学 Method for preparing α type high-strength gypsum by microwave irradiation of phosphogypsum crystal transformation under normal pressure
CN111716536A (en) * 2020-06-28 2020-09-29 浙江古思建筑科技有限公司 Production process of gypsum self-leveling material
CN113372083A (en) * 2021-07-19 2021-09-10 福泉环保城发展有限公司 Graphene oxide based layered material modified self-leveling mortar and preparation method thereof
CN113896500A (en) * 2021-09-27 2022-01-07 贵州恒源科创资源再生开发有限公司 Preparation method of sand-free paste-based self-leveling slurry
CN118619569A (en) * 2024-08-12 2024-09-10 米脂冀东水泥有限公司 Method for manufacturing oil well cement by using magnesium slag

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CN109824292A (en) * 2019-03-26 2019-05-31 菲大装配式建筑工程(重庆)有限责任公司 A kind of graphene-based composite material and preparation method, application
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CN113896500A (en) * 2021-09-27 2022-01-07 贵州恒源科创资源再生开发有限公司 Preparation method of sand-free paste-based self-leveling slurry
CN118619569A (en) * 2024-08-12 2024-09-10 米脂冀东水泥有限公司 Method for manufacturing oil well cement by using magnesium slag

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